Pavement rubber asphalt crack pouring adhesive and preparation method thereof

By double surface modification of nano-silica, the interface compatibility and adhesion of the seam filling glue are enhanced, the stability of seam filling glue in high and low temperature environments is solved, and the high temperature stability and mechanical properties are improved.

CN120484778AActive Publication Date: 2025-08-15WEIFANG HIGHWAY DEV GRP CO LTD

Patent Information

Application Number
CN202510917179.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-03
Publication Date
2025-08-15
Estimated Expiration
2045-07-03

AI Technical Summary

Technical Problem

The existing seam filling glue reduces viscoelasticity at high temperatures, softens and flow, and the rigidity rises sharply at low temperatures, and brittle fractures easily. The uneven dispersion of nanoparticles leads to stress concentration, affecting the stability and life of the material.

Method used

The nanosilica was double surface modification by α-octadecene and sulfobetaine methacrylate. By introducing long-chain alkyl and sulfobetaine groups, the interface compatibility and adhesion with asphalt and rubber powder are enhanced, and a physical crosslinking network is formed to improve high temperature stability and mechanical properties.

Benefits of technology

Significantly improve the high temperature stability and mechanical properties of the seam filling glue, enhance the adhesion with the crack surface, prevent peeling, and meet the material stability needs in complex environments.

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Abstract

The invention relates to the technical field of rubber asphalt, in particular to a pavement rubber asphalt crack pouring adhesive and a preparation method thereof. The pavement rubber asphalt crack pouring adhesive is prepared from the following components in parts by mass: asphalt, rubber powder, a compatilizer, modified silicon dioxide, a silane coupling agent and an auxiliary agent, according to the pavement rubber asphalt crack pouring adhesive, asphalt, rubber powder and modified silicon dioxide are compounded; the preparation method comprises the following steps: treating nano silicon dioxide by adopting a KH570 silane coupling agent, introducing unsaturated double bonds into the nano silicon dioxide, then carrying out free radical polymerization on the nano silicon dioxide, alpha-octadecene and sulfobetaine methacrylate under the catalysis of BPO, and respectively introducing long-chain alkyl, sulfo and betaine groups into the modified nano silicon dioxide, so as to obtain the modified nano silicon dioxide. The interfacial compatibility among the components is improved, so that the high-temperature stability and the mechanical property of the crack pouring adhesive are improved.
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Description

Technical Field

[0001] The present invention relates to the technical field of rubber asphalt, in particular to a pavement rubber asphalt joint filling glue and a preparation method thereof. Background Art

[0002] Asphalt pavement crack caulking adhesive is the core material for pavement crack repair, and its performance directly determines the pavement's resistance to damage and service life. Traditional caulking adhesives are usually based on asphalt, and their temperature sensitivity and mechanical properties are adjusted by adding rubber powder or thermoplastic elastomers (such as SBS). However, this type of material has significant defects in practical applications: under high temperature environments, the viscoelasticity of the asphalt matrix decreases, causing the caulking adhesive to soften or even flow, making it difficult to maintain its sealing effect on the cracks; under low temperature conditions, the material's rigidity increases sharply, its ductility decreases, and it is prone to brittle fracture. This is especially true in areas with large temperature differences between day and night or drastic seasonal climates. Repeated thermal expansion and contraction will accelerate interfacial delamination, ultimately causing secondary cracking. In addition, the existing solution of excessively increasing the SBS content to improve high-temperature stability not only significantly increases costs, but also exacerbates the problem of elastic failure after UV aging. Under long-term exposure, the material surface will obviously powder and harden, and the bond strength decay rate will exceed 40%.

[0003] In recent years, the introduction of nanofillers has been recognized as a key approach to improving the performance of caulking adhesives. For example, nanosilica, due to its high specific surface area and surface activity, can effectively enhance the material's mechanical strength and thermal stability. However, in conventional processes, nanoparticles easily agglomerate into micron-sized particles due to the surface energy difference with the asphalt matrix. This not only weakens the reinforcing effect but also creates stress concentration points within the material, inducing microcrack propagation under dynamic loading. To address the dispersion issue, existing technologies often utilize single silane coupling agents (such as KH550 and KH570) to surface modify nanosilica. However, these mechanisms of action are limited to physical coating or simple chemical bonding. In complex environments (such as heat and humidity, and freeze-thaw cycles), the coupling agent's molecular chains are susceptible to hydrolysis or cleavage, leading to debonding between the nanoparticles and the matrix. Furthermore, some modification processes require high temperatures, prolonged reactions, or the use of large amounts of organic solvents. This not only consumes a lot of energy but also releases volatile organic compounds, which is inconsistent with current industry demands for green and environmentally friendly materials. Therefore, breakthroughs are urgently needed through innovative material design and process optimization. Summary of the Invention

[0004] Based on this, it is necessary to provide a pavement rubber asphalt caulking glue. The present invention uses α-octadecene and sulfobetaine methacrylate to perform double surface modification on nano-silica, which significantly improves the interface bonding strength and temperature stability.

[0005] One object of the present invention is to provide a pavement rubber asphalt joint filling glue, comprising the following components in parts by mass: 60-75 parts asphalt 10-30 parts rubber powder 20-30 parts of compatibilizer 10-15 parts of modified silica 1-3 parts silane coupling agent 1-15 parts of auxiliary agent; The modified silicon dioxide is obtained by reacting α-octadecene, sulfobetaine methacrylate and nano silicon dioxide treated with KH570.

[0006] Furthermore, the asphalt is selected from one or more of petroleum asphalt, natural asphalt, and blended asphalt.

[0007] Furthermore, the particle size of the rubber powder is 20-80 mesh.

[0008] Furthermore, the silane coupling agent is selected from one or more of A151, A171, and A172.

[0009] Furthermore, the compatibilizer is selected from one or more of naphthenic oil, aromatic oil and oil extracted from the third line.

[0010] Furthermore, the auxiliary agent is selected from one or more of a stabilizer and a rubber vulcanizing agent.

[0011] Furthermore, the rubber vulcanizing agent is selected from one or more of sulfur, rubber accelerator D, TMTD or rubber accelerator M.

[0012] The present invention also provides a method for preparing the pavement rubber asphalt crack filling glue, which comprises the following steps: S1. Under the protection of inert gas, nano-silica and KH570 are mixed and heated to react to obtain an intermediate product; S2. Under the protection of an inert gas, the intermediate product, α-octadecene, and sulfobetaine methacrylate are blended, an initiator is added, and the mixture is heated for reaction to obtain modified silica; S3. Evenly mix the modified silicon dioxide with other ingredients, heat and shear in a high-speed shear emulsifier to obtain a pavement rubber asphalt joint sealant.

[0013] Furthermore, in step S1, the temperature of the heating reaction is 100-110°C.

[0014] Furthermore, in step S2, the temperature of the heating reaction is 75-85°C.

[0015] The present invention has the following beneficial effects: The pavement rubber asphalt caulking glue of the present invention is compounded with asphalt, rubber powder and modified silica. First, nano silica is treated with KH570 silane coupling agent to introduce unsaturated double bonds into the nano silica. Then, free radical polymerization is carried out with α-octadecene and sulfobetaine methacrylate under the catalysis of BPO to introduce long-chain alkyl, sulfo and betaine groups into the modified nano silica respectively. On the one hand, since the modified nano silica introduces the long alkyl chain of octadecene, the interface characteristics of the modified nano silica are effectively adjusted, the compatibility between the modified nano silica and the asphalt and rubber powder is improved, and the agglomeration of the modified nano silica is avoided. In addition, the long-chain alkyl can It can be entangled and cross-linked with asphalt or rubber powder through molecular entanglement to form a physical cross-linking network, thereby improving the interfacial compatibility between the components, thereby improving the high-temperature stability and mechanical properties of the caulking adhesive; secondly, since the modified nano-silica also introduces hydrophilic groups such as sulfonic groups and betaine groups, the sulfonic groups can form hydrogen bonds with polar groups such as oxygen-containing groups in asphalt, further enhancing the interfacial bonding force between the components, and the flexible chain segments of betaine can improve the elasticity of the caulking adhesive and improve the tensile strength of the caulking adhesive; in addition, due to the hydrophilic properties of the sulfonic and betaine groups, the adhesion between the caulking adhesive and the crack surface (especially the wet base surface) can be enhanced, preventing the caulking adhesive from peeling off, and significantly improving the mechanical properties of the caulking adhesive. DETAILED DESCRIPTION

[0016] In order to more clearly illustrate the technical solutions of the present invention, the following examples are given. Unless otherwise stated, the raw materials, reactions and post-processing methods mentioned in the examples are common raw materials on the market and technical methods well known to those skilled in the art.

[0017] The terms "preferred," "preferably," "more preferred," and the like, used herein, refer to embodiments of the invention that may provide certain benefits under certain circumstances. However, other embodiments may also be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.

[0018] It should be understood that, except in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about." Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and appended claims are approximations that may vary depending upon the desired properties to be obtained by the present invention.

[0019] Asphalt, AH-90 petroleum asphalt, was purchased from Hebei Dezhishan Petrochemical Co., Ltd.

[0020] Rubber powder, 40 mesh, was purchased from Lingshou County Yiteng New Material Technology Co., Ltd.

[0021] Silane coupling agent, A151, vinyltriethoxysilane.

[0022] Compatibilizer, minus three-line extraction oil, 100SN, was purchased from Shenzhen Huameite Lubrication Technology Co., Ltd.

[0023] Stabilizer, chromic anhydride.

[0024] Rubber vulcanizing agent, rubber accelerator M, 2-mercaptobenzothiazole were purchased from Nanjing Reagent.

[0025] Sultaine methacrylate, 537284, was purchased from Sigma.

[0026] KH570, γ-methacryloxypropyltrimethoxysilane.

[0027] BPO, benzoyl peroxide.

[0028] Example 1 A pavement rubber asphalt joint filling glue, comprising the following components in parts by weight: 63 parts asphalt 15 parts rubber powder 23 parts of compatibilizer 11 parts of modified silica 1 part silane coupling agent 1 part stabilizer 3 parts of rubber vulcanizing agent; The preparation method of the above-mentioned road rubber asphalt caulking glue comprises the following steps: S1. In parts by weight, 10 parts of nano-silica and 3 parts of KH570 were mixed in 80 parts of toluene under nitrogen, and ultrasonically dispersed for 30 minutes. The mixture was heated to 110°C and reacted for 5 hours. After filtering, the mixture was washed with deionized water three times and dried to obtain an intermediate product. S2, adding 5 parts of the intermediate product, 10 parts of α-octadecene and 5 parts of sulfobetaine methacrylate to 80 parts of toluene, adding 1 part of BPO as a catalyst under nitrogen protection, reacting at 80° C. for 5 hours, cooling, filtering, washing with deionized water 3 times, and drying to obtain the modified silica; S3. According to the above-mentioned mass fractions, evenly mix the modified silica with other ingredients except the stabilizer and rubber vulcanizer, add them into a high-speed shear emulsifier, shear at a shear temperature of 160°C for 45 minutes, then add the stabilizer and rubber vulcanizer, and stir at this temperature for 50 minutes to obtain the pavement rubber asphalt caulking glue.

[0029] Example 2 A pavement rubber asphalt joint filling glue, comprising the following components in parts by weight: 66 parts asphalt 17 parts rubber powder 25 parts of compatibilizer 12 parts of modified silica 2 parts of silane coupling agent 1 part stabilizer 3 parts of rubber vulcanizing agent; The preparation method of the above-mentioned road rubber asphalt caulking glue comprises the following steps: S1. In parts by weight, 10 parts of nano-silica and 3 parts of KH570 were mixed in 80 parts of toluene under nitrogen, and ultrasonically dispersed for 30 minutes. The mixture was heated to 110°C and reacted for 5 hours. After filtering, the mixture was washed with deionized water three times and dried to obtain an intermediate product. S2, adding 5 parts of the intermediate product, 10 parts of α-octadecene and 5 parts of sulfobetaine methacrylate to 80 parts of toluene, adding 1 part of BPO as a catalyst under nitrogen protection, reacting at 80° C. for 5 hours, cooling, filtering, washing with deionized water 3 times, and drying to obtain the modified silica; S3. According to the above-mentioned mass fractions, evenly mix the modified silica with other ingredients except the stabilizer and rubber vulcanizer, add them into a high-speed shear emulsifier, shear at a shear temperature of 160°C for 45 minutes, then add the stabilizer and rubber vulcanizer, and stir at this temperature for 50 minutes to obtain the pavement rubber asphalt caulking glue.

[0030] Example 3 A pavement rubber asphalt joint filling glue, comprising the following components in parts by weight: 70 parts asphalt 18 parts rubber powder 27 parts of compatibilizer 14 parts modified silica 2 parts of silane coupling agent 1 part stabilizer 3 parts of rubber vulcanizing agent; The preparation method of the above-mentioned road rubber asphalt caulking glue comprises the following steps: S1. In parts by weight, 10 parts of nano-silica and 3 parts of KH570 were mixed in 80 parts of toluene under nitrogen, and ultrasonically dispersed for 30 minutes. The mixture was heated to 110°C and reacted for 5 hours. After filtering, the mixture was washed with deionized water three times and dried to obtain an intermediate product. S2, adding 5 parts of the intermediate product, 10 parts of α-octadecene and 5 parts of sulfobetaine methacrylate to 80 parts of toluene, adding 1 part of BPO as a catalyst under nitrogen protection, reacting at 80° C. for 5 hours, cooling, filtering, washing with deionized water 3 times, and drying to obtain the modified silica; S3. According to the above-mentioned mass fractions, evenly mix the modified silica with other ingredients except the stabilizer and rubber vulcanizer, add them into a high-speed shear emulsifier, shear at a shear temperature of 160°C for 45 minutes, then add the stabilizer and rubber vulcanizer, and stir at this temperature for 50 minutes to obtain the pavement rubber asphalt caulking glue.

[0031] Comparative Example 1 A crack filling glue is disclosed. The difference between this comparative example and Example 1 is that in step S2, α-octadecene is removed and only sulfobetaine methacrylate is used to react with the intermediate product. Other components and preparation methods are the same.

[0032] Comparative Example 2 A crack filling glue is disclosed. The difference between this comparative example and Example 1 is that in step S2, butyl acrylate of equal mass is used to replace sulfobetaine methacrylate, and other components and preparation methods are the same.

[0033] Comparative Example 3 A kind of caulking glue, brand number 20241022, was purchased from Dongping Dingxiang New Materials Center.

[0034] Test Case The performance of the caulking glue prepared in Example 1 and Comparative Examples 1-2 was tested.

[0035] The test was conducted in accordance with the standard of ordinary type in 5.2 of JT-T2009-740 "Standard for Sealant for Cracks in Asphalt Pavement".

[0036] The test results are shown in Table 1.

[0037] Table 1 Performance test results of the caulking glue of Example 1 and Comparative Examples 1-2 Test items Example 1 Comparative Example 1 Comparative Example 2 Comparative Example 3 Low temperature stretching pass 1 failed pass 2 failed Cone penetration (0.1mm) 67 59 63 57 Softening point (%) 97 91 93 88 Flow value (mm) 0.6 0.9 0.7 1.3 Elastic recovery rate (%) 76 68 73 61 According to Table 1, it can be concluded that the caulking glue of the present invention has better bonding performance, resilience and temperature stability. The caulking glue of Example 1 has excellent comprehensive performance, and its low-temperature flexibility, high-temperature stability (high softening point, low flow value) and elastic recovery ability are all outstanding, which fully meets the standard requirements; while Comparative Examples 1 and 3 have key defects such as unqualified low-temperature performance or poor high-temperature flow resistance, and the performance of Comparative Example 2 is inferior to that of Example 1 in all aspects.

[0038] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0039] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A pavement rubber asphalt joint filling glue, characterized in that: The composition includes the following components in parts by weight: 60-75 parts asphalt 10-30 parts rubber powder 20-30 parts of compatibilizer 10-15 parts of modified silica 1-3 parts silane coupling agent 1-15 parts of auxiliary agent; The modified silicon dioxide is obtained by reacting α-octadecene, sulfobetaine methacrylate and nano silicon dioxide treated with KH570.

2. The road rubber asphalt joint filling glue according to claim 1 is characterized in that: The asphalt is selected from one or more of petroleum asphalt, natural asphalt, and blended asphalt.

3. The road rubber asphalt joint filling glue according to claim 1 is characterized in that: The particle size of the rubber powder is 20-80 meshes.

4. The road rubber asphalt joint filling glue according to claim 1, characterized in that: The compatibilizer is selected from one or more of naphthenic oil, aromatic oil and oil extracted from the third subtraction line.

5. The road rubber asphalt joint filling glue according to claim 1 is characterized in that: The silane coupling agent is selected from one or more of A151, A171, and A172.

6. The road rubber asphalt joint filling glue according to claim 1, characterized in that: The auxiliary agent is selected from one or more of a stabilizer and a rubber vulcanizing agent.

7. The road rubber asphalt joint filling glue according to claim 1 is characterized in that: The rubber vulcanizing agent is selected from one or more of sulfur, rubber accelerator D, TMTD or rubber accelerator M.

8. The method for preparing the pavement rubber asphalt joint sealant according to any one of claims 1 to 7, characterized in that: The preparation method of the pavement rubber asphalt crack filling glue comprises the following steps: S1. Under the protection of inert gas, nano-silica and KH570 are mixed and heated to react to obtain an intermediate product; S2. Under the protection of an inert gas, the intermediate product, α-octadecene, and sulfobetaine methacrylate are blended, an initiator is added, and the mixture is heated for reaction to obtain modified silica; S3. Evenly mix the modified silicon dioxide with other ingredients, heat and shear in a high-speed shear emulsifier to obtain a pavement rubber asphalt joint sealant.

9. The method for preparing the pavement rubber asphalt crack filling glue according to claim 8, characterized in that: In step S1, the temperature of the heating reaction is 100-110°C.

10. The method for preparing the road rubber asphalt joint filling glue according to claim 8, characterized in that: In step S2, the temperature of the heating reaction is 75-85°C.

Citation Information

Patent Citations

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  • High-performance rubber asphalt pouring sealant and preparation method thereof

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  • Asphalt pavement crack filling adhesive and preparation method thereof

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    CN105218720A

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